EP1029907B1 - Process for mechanical chemical polishing of a layer of aluminium or aluminium alloy conducting material - Google Patents

Process for mechanical chemical polishing of a layer of aluminium or aluminium alloy conducting material Download PDF

Info

Publication number
EP1029907B1
EP1029907B1 EP00810129A EP00810129A EP1029907B1 EP 1029907 B1 EP1029907 B1 EP 1029907B1 EP 00810129 A EP00810129 A EP 00810129A EP 00810129 A EP00810129 A EP 00810129A EP 1029907 B1 EP1029907 B1 EP 1029907B1
Authority
EP
European Patent Office
Prior art keywords
aluminium
process according
colloidal silica
abrasive
composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP00810129A
Other languages
German (de)
French (fr)
Other versions
EP1029907A1 (en
Inventor
Eric Jacquinot
Pascal Letourneau
Maurice Rivoire
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
EMD Performance Materials Corp
Original Assignee
Clariant Finance BVI Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Clariant Finance BVI Ltd filed Critical Clariant Finance BVI Ltd
Publication of EP1029907A1 publication Critical patent/EP1029907A1/en
Application granted granted Critical
Publication of EP1029907B1 publication Critical patent/EP1029907B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321After treatment
    • H01L21/32115Planarisation
    • H01L21/3212Planarisation by chemical mechanical polishing [CMP]
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions

Definitions

  • the present invention relates to a process for mechanical chemical polishing of a layer of an aluminium or aluminium alloy conducting material used in the microelectronics industry for semi-conductors as material which constitutes interconnecting tracks.
  • interconnecting tracks Electronic devices made on a silicon slice must be connected to each other by means of interconnecting tracks to constitute the desired electronic circuit.
  • these interconnecting tracks are most often defined using an aluminium-based film.
  • the aluminium can be associated with silicon or (and) copper in weak proportions in order to increase its resistance to electromigration.
  • the interconnecting tracks of semi-conductors are usually made according to the following sequence: an aluminium or aluminium alloy film approximately 1 ⁇ m thick is deposited by bombardment of an aluminium or aluminium alloy target by means of a beam of electrons or beam of ions (sputtering); the design of the interconnecting circuit is then transferred there by photolithography then by reactive ionic etching (RIE).
  • RIE reactive ionic etching
  • the tracks thus defined must be electrically isolated, they are also covered with a dielectric layer, usually based on silicon oxide, most often obtained by decomposition in the vapor phase of tetraethylorthosilicate (TEOS). This layer is then planarized by mechanical chemical polishing.
  • the damascene process constitutes an alternative solution which allows interconnecting tracks to be made of aluminium whilst reducing the number of stages required. It consists of depositing a silicon oxide based dielectric layer on a substrate. In this dielectric layer, the contact holes and trenches which reproduce the design of the interconnecting circuit are then formed by two photolithographies and successive reactive ionic etchings. An aluminium or aluminium alloy layer is then deposited, which is polished by mechanical chemical polishing until the surface of the dielectric layer is reached. The aluminium thus remains only in the contacts and the trenches.
  • the damascene process allow problems linked to the reactive ionic etching of aluminium to be avoided: poor selectivity of aluminium etching compared with its counter-mask in resin and difficult control of the profile of aluminium tracks.
  • aluminium polishing stage should thus not only be uniform but also result in an excellent surface state.
  • aluminium is a soft and malleable metal which is difficult to polish without scratches.
  • EP-A-0 779 655 It was proposed in EP-A-0 779 655 to use an abrasive composition comprising a suspension of fumed silica for polishing aluminium or aluminium alloy surfaces.
  • WO-A-97/13889 describes a process intended for polishing aluminium, copper, nickel or tantalum films using an abrasive solution comprising a suspension of aluminium oxide particles.
  • EP-A-0 520 109 describes a primary polishing process for silicon trenches using a composition comprised of a colloidal solution of silica stabilized by ammonium hydroxide, a bactericide of the quaternary ammonium hydroxide family, and up to 0.1% by weight of chlorite or sodium hypochlorite.
  • EP-A-0 853 335 describes a selective polishing process between a silicon oxide layer and a silicon nitride layer using a modified slurry obtained by combining a slurry with a tetramethylammonium salt, a base and hydrogen peroxide, in which the ratio by volume of slurry to hydrogen peroxide is high, particularly comprised between 200 and 500 to 1.
  • EP-A-0 896 042 describes a mechanical chemical polishing composition
  • a compound capable of attacking tungsten such as hydrogen peroxide and at least one tungsten attack inhibitor such as tetraalkylammonium hydroxide, and the pH of which is less than 7.
  • a subject of the present invention is therefore a process for mechanical chemical polishing of a layer of an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry, characterized in that a layer of said material is abraded using an abrasive composition comprising an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetralkylammonium hydroxide and an oxidizing agent.
  • the oxidizing agent is responsible for improving the polishing properties of abrasive compositions of the invention, whilst the tetraalkylammonium hydroxide stabilizes the composition.
  • the abrasive compositions used according to the invention will notably have a pH comprised between 8 and 12, preferably between 10.5 and 11.
  • abrasive compositions can be obtained, for example, using a silica colloidal solution stabilized with sodium.
  • This colloidal solution of silica will thus be treated on a cation exchange resin to eliminate the sodium present, then by tetramethylammonium hydroxide to obtain a stable alkaline aqueous suspension, a subject of the present invention.
  • Abrasive compositions advantageous for use according to the invention are obtained using colloidal silica with individualized particles, not linked to each other by siloxane bonds and having average particle diameters comprised between 12 nm and 100 nm, preferably between 35 nm and 50 nm and very particularly of approximately 50 nm.
  • the abrasive particles are advantageously present in a concentration by weight comprised between 5% and 50%, preferably between 25% and 35%, and very particularly in a concentration of approximately 30%.
  • the tetraalkylammonium hydroxide used to stabilize the abrasive compositions according to the invention is preferably chosen from tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide and most particularly tetramethylammonium hydroxide.
  • This tetraalkylammonium hydroxide could preferably be used at a concentration comprised between 0.1% by weight and 1% by weight relative to the initial silica and most particularly at a concentration of approximately 0.4% by weight relative to the initial silica.
  • the abrasive compositions used in the invention preferably contain between 0.5% and 10% by volume of oxidizing agent.
  • oxidizing agent is notably chosen from chlorates, perchlorates, chlorites, iodates, nitrates, sulphates, persulphates, peroxides, ozonized water and hydrogen peroxide.
  • the oxidizing agent will preferably be hydrogen peroxide.
  • a preferred composition above is characterized in that the quantity of hydrogen peroxide diluted to 30% present in said abrasive composition is comprised between 0.5% and 10% by volume relative to the total of said abrasive composition and notably is approximately 7.5% by volume relative to the total of said abrasive composition.
  • compositions used in the invention have remarkable properties which justify their use in the polishing of a layer in an aluminium or aluminium alloy based conducting material, being able to be for example an aluminium-copper alloy or an aluminium-silicon-copper alloy.
  • a subject of the present Application is the use of an abrasive composition
  • an abrasive composition comprising an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetraalkylammonium hydroxide and an oxidizing agent for mechanical chemical polishing an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry.
  • Example of mechanical chemical polishing with an abrasive identical to that of example 1, without the addition of hydrogen peroxide Using slices identical to those in example 2 and under the same operating conditions as those in example 2 and using an alkaline aqueous suspension of colloidal silica stabilized by 0.4% by weight of tetramethylammonium hydroxide, the characteristics of which are the following:
  • this suspension generates numerous scratches on the surface of the aluminium. This poor surface state forbids the use of this process for making interconnecting tracks in aluminium using the damascene process.
  • Example of mechanical chemical polishing with an abrasive comprising an alkaline aqueous suspension of colloidal silica stabilized by 1.2% by weight of NH 3 (Klebosol® 30 N 50 PHN from Clariant France SA) and comprising 7.5% by volume of hydrogen peroxide diluted to 30%.
  • NH 3 Kelbosol® 30 N 50 PHN from Clariant France SA
  • Example of mechanical chemical polishing with an abrasive comprising an acidic aqueous suspension of colloidal silica (Klebosol® 30 H 50 from Clariant France SA) and 7.5% by volume of hydrogen peroxide diluted to 30%.
  • an acidic aqueous suspension of colloidal silica the characteristics of which are the following:

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Conductive Materials (AREA)
  • ing And Chemical Polishing (AREA)
  • Polishing Bodies And Polishing Tools (AREA)
  • Chemically Coating (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Non-Insulated Conductors (AREA)

Abstract

Process for mechanical chemical polishing of a layer of an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry in which said aluminium or aluminium alloy layer is abraded using an abrasive composition which comprises an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetraalkylammonium hydroxide and an oxidizing agent.

Description

  • The present invention relates to a process for mechanical chemical polishing of a layer of an aluminium or aluminium alloy conducting material used in the microelectronics industry for semi-conductors as material which constitutes interconnecting tracks.
  • Electronic devices made on a silicon slice must be connected to each other by means of interconnecting tracks to constitute the desired electronic circuit. Currently, these interconnecting tracks are most often defined using an aluminium-based film. The aluminium can be associated with silicon or (and) copper in weak proportions in order to increase its resistance to electromigration.
  • The interconnecting tracks of semi-conductors are usually made according to the following sequence: an aluminium or aluminium alloy film approximately 1 µm thick is deposited by bombardment of an aluminium or aluminium alloy target by means of a beam of electrons or beam of ions (sputtering); the design of the interconnecting circuit is then transferred there by photolithography then by reactive ionic etching (RIE). The tracks thus defined must be electrically isolated, they are also covered with a dielectric layer, usually based on silicon oxide, most often obtained by decomposition in the vapor phase of tetraethylorthosilicate (TEOS). This layer is then planarized by mechanical chemical polishing.
  • The damascene process constitutes an alternative solution which allows interconnecting tracks to be made of aluminium whilst reducing the number of stages required. It consists of depositing a silicon oxide based dielectric layer on a substrate. In this dielectric layer, the contact holes and trenches which reproduce the design of the interconnecting circuit are then formed by two photolithographies and successive reactive ionic etchings. An aluminium or aluminium alloy layer is then deposited, which is polished by mechanical chemical polishing until the surface of the dielectric layer is reached. The aluminium thus remains only in the contacts and the trenches.
  • The damascene process allow problems linked to the reactive ionic etching of aluminium to be avoided: poor selectivity of aluminium etching compared with its counter-mask in resin and difficult control of the profile of aluminium tracks.
  • To carry out mechanical chemical polishing of the aluminium or aluminium alloy layer, two phenomena must be avoided:
    • an attack on the subjacent silicon oxide layer, also called erosion. This introduces ridges locally and is counter-productive to the desired aim of planarization.
    • an over-polishing of the interconnecting lines in the trenches, also called "dishing". Not only does this phenomenon also generate ridges, but also reduces the thickness of the interconnecting lines, and for this reason, increases their resistance.
  • These two phenomena are mainly due to a poor polishing uniformity of the aluminium or aluminium alloy. In fact, an imperfect removal of the metallic layer generally imposes significant over-polishing to avoid any risk of electric conduction between the different electronic devices, which leads to over-polishing the interconnecting lines and the dielectric zones already revealed.
  • The aluminium polishing stage should thus not only be uniform but also result in an excellent surface state. In fact, aluminium is a soft and malleable metal which is difficult to polish without scratches.
  • These scratches can be generated in two main ways:
    • aluminium oxide, which forms naturally on the surface of aluminium, is a harder material than aluminium. The particles of this aluminium oxide layer, once abraded, can agglomerate then scratch the surface of the aluminium. An abrasive composition must thus be used which minimizes the formation of surface aluminium oxide and/or avoids the agglomeration of abraded aluminium oxide particles,
    • the particles which constitute the abrasive composition can also scratch the surface of the aluminium if their form and their roughness are badly controlled, which favors the colloidal suspensions of silica more than abrasives based on fumed silica or aluminium oxide.
  • It was proposed in EP-A-0 779 655 to use an abrasive composition comprising a suspension of fumed silica for polishing aluminium or aluminium alloy surfaces.
  • WO-A-97/13889 describes a process intended for polishing aluminium, copper, nickel or tantalum films using an abrasive solution comprising a suspension of aluminium oxide particles.
  • At a different stage of manufacturing electronic circuits, very much upstream, EP-A-0 520 109 describes a primary polishing process for silicon trenches using a composition comprised of a colloidal solution of silica stabilized by ammonium hydroxide, a bactericide of the quaternary ammonium hydroxide family, and up to 0.1% by weight of chlorite or sodium hypochlorite.
  • At yet another different stage of manufacturing electronic circuits, EP-A-0 853 335 describes a selective polishing process between a silicon oxide layer and a silicon nitride layer using a modified slurry obtained by combining a slurry with a tetramethylammonium salt, a base and hydrogen peroxide, in which the ratio by volume of slurry to hydrogen peroxide is high, particularly comprised between 200 and 500 to 1.
  • EP-A-0 896 042 describes a mechanical chemical polishing composition comprising a compound capable of attacking tungsten such as hydrogen peroxide and at least one tungsten attack inhibitor such as tetraalkylammonium hydroxide, and the pH of which is less than 7.
  • The abrasives currently known and intended for polishing aluminium or aluminium alloy, being essentially aluminium or fumed silica based abrasives, do not allow a satisfactory surface quality to be obtained.
  • Now, the Applicant has noted in surprising and unexpected fashion that the use of an alkaline aqueous suspension of colloidal silica stabilized by a tetraalkylammonium hydroxide and associated with a oxidizing agent allowed:
    • an increased polishing speed for an aluminium or aluminium alloy plate,
    • an excellent aluminium surface state.
  • A subject of the present invention is therefore a process for mechanical chemical polishing of a layer of an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry, characterized in that a layer of said material is abraded using an abrasive composition comprising an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetralkylammonium hydroxide and an oxidizing agent.
  • According to research carried out by the Applicant, the oxidizing agent is responsible for improving the polishing properties of abrasive compositions of the invention, whilst the tetraalkylammonium hydroxide stabilizes the composition.
  • The abrasive compositions used according to the invention will notably have a pH comprised between 8 and 12, preferably between 10.5 and 11.
  • These abrasive compositions can be obtained, for example, using a silica colloidal solution stabilized with sodium. This colloidal solution of silica will thus be treated on a cation exchange resin to eliminate the sodium present, then by tetramethylammonium hydroxide to obtain a stable alkaline aqueous suspension, a subject of the present invention.
  • Abrasive compositions advantageous for use according to the invention are obtained using colloidal silica with individualized particles, not linked to each other by siloxane bonds and having average particle diameters comprised between 12 nm and 100 nm, preferably between 35 nm and 50 nm and very particularly of approximately 50 nm.
  • In all the compositions used according to the invention, the abrasive particles are advantageously present in a concentration by weight comprised between 5% and 50%, preferably between 25% and 35%, and very particularly in a concentration of approximately 30%.
  • The tetraalkylammonium hydroxide used to stabilize the abrasive compositions according to the invention is preferably chosen from tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide and most particularly tetramethylammonium hydroxide.
  • This tetraalkylammonium hydroxide could preferably be used at a concentration comprised between 0.1% by weight and 1% by weight relative to the initial silica and most particularly at a concentration of approximately 0.4% by weight relative to the initial silica.
  • The abrasive compositions used in the invention preferably contain between 0.5% and 10% by volume of oxidizing agent. This is notably chosen from chlorates, perchlorates, chlorites, iodates, nitrates, sulphates, persulphates, peroxides, ozonized water and hydrogen peroxide.
  • The oxidizing agent will preferably be hydrogen peroxide. A preferred composition above is characterized in that the quantity of hydrogen peroxide diluted to 30% present in said abrasive composition is comprised between 0.5% and 10% by volume relative to the total of said abrasive composition and notably is approximately 7.5% by volume relative to the total of said abrasive composition.
  • The compositions used in the invention have remarkable properties which justify their use in the polishing of a layer in an aluminium or aluminium alloy based conducting material, being able to be for example an aluminium-copper alloy or an aluminium-silicon-copper alloy.
  • Finally, a subject of the present Application is the use of an abrasive composition comprising an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetraalkylammonium hydroxide and an oxidizing agent for mechanical chemical polishing an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry.
  • Preferred conditions of using the polishing processes described above also apply to the other subjects of the invention envisaged above.
  • The scope of the invention can be understood better by referring to the examples given below, the aim of which is to explain the advantages of the invention.
  • EXAMPLE 1: Abrasive composition
  • 7.5% by volume of hydrogen peroxide diluted to 30% is added to a suspension of colloidal silica stabilized by 0.4% by weight of tetramethylammonium hydroxide (sample PL 1509 from Clariant France SA), the characteristics of which are as follows:
    • pH of the aqueous suspension: 11
    • specific surface: 55 m2/g
    • average diameter of the elementary particles of colloidal silica: 50 nm
    • concentration by weight in colloidal silica: 30%
  • An abrasive composition according to the invention is thus obtained.
  • EXAMPLE 2: Example of mechanical chemical polishing
  • On each plate studied, aluminium of 10000 Å thickness is deposited on a layer of 1600 Å silicon oxide. The slices are then polished on a PRESI E 460 polisher with the following polishing conditions:
    • applied pressure 0.2 daN/cm2
    • turntable speed 30 rpm
    • head speed 30 rpm
    • abrasive temperature 20°C
    • abrasion rate 100 cm3/mn
    • fabric IC 1000 furrows from Rodel Products
    using an abrasive obtained in example 1. This abrasive composition allows the following results to be obtained:
    • an aluminium polishing speed of 1700 Å/mn,
    • an excellent surface state (no scratches observed under the optical microscope),
    • a polishing non-uniformity equal to 8%.
    COMPARISON EXAMPLE 1
  • Example of mechanical chemical polishing with an abrasive identical to that of example 1, without the addition of hydrogen peroxide. Using slices identical to those in example 2 and under the same operating conditions as those in example 2 and using an alkaline aqueous suspension of colloidal silica stabilized by 0.4% by weight of tetramethylammonium hydroxide, the characteristics of which are the following:
    • pH of the aqueous suspension: 11
    • specific surface: 55 m2/g
    • average diameter of elemental particles of colloidal silica: 50 nm
    • concentration by weight in colloidal silica: 30 %
    the following results are obtained:
    • an aluminium polishing speed of 1450 Å/mn,
    • a polishing non-uniformity equal to 15%.
  • Moreover, this suspension generates numerous scratches on the surface of the aluminium. This poor surface state forbids the use of this process for making interconnecting tracks in aluminium using the damascene process.
  • COMPARISON EXAMPLE 2
  • Example of mechanical chemical polishing with an abrasive comprising an alkaline aqueous suspension of colloidal silica stabilized by 1.2% by weight of NH3 (Klebosol® 30 N 50 PHN from Clariant France SA) and comprising 7.5% by volume of hydrogen peroxide diluted to 30%. Using slices identical to those in example 2 and under the same operating conditions as those in example 2, and using an alkaline aqueous suspension of colloidal silica stabilized by 1.2% by weight of NH3, the characteristics of which are as follows:
    • pH of the aqueous suspension: 11
    • specific surface: 57 m2/g
    • average diameter of the elemental particles of colloidal silica: 50 nm
    • concentration by weight in colloidal silica: 30%
    to which 7.5% by volume of hydrogen peroxide diluted to 30% is added, the following results are obtained:
    • an aluminium polishing speed of 1600 Å/mn,
    • a polishing non-uniformity equal to 10%.
  • However, it generates numerous scratches on the surface of the aluminium. This poor surface state forbids the use of this process for making interconnecting tracks in aluminium by the damascene process.
  • COMPARISON EXAMPLE 3
  • Example of mechanical chemical polishing with an abrasive comprising an acidic aqueous suspension of colloidal silica (Klebosol® 30 H 50 from Clariant France SA) and 7.5% by volume of hydrogen peroxide diluted to 30%. Using slices identical to those in example 2 and under the same operating conditions as those of example 2, using an acidic aqueous suspension of colloidal silica, the characteristics of which are the following:
    • pH of the aqueous suspension: 2.2
    • specific surface: 54 m2/g
    • average diameter of the elemental particles of colloidal silica: 50 nm
    • concentration by weight in colloidal silica: 30%
    to which 7.5% by volume of hydrogen peroxide diluted to 30% is added, numerous scratches on the surface of the aluminium are generated. This poor surface state thus forbids the use of the process for making interconnecting tracks in aluminium by the damascene process.

Claims (15)

  1. A process for mechanical chemical polishing of a layer of an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry, characterized in that said aluminium or aluminium alloy layer is abraded using an abrasive composition which comprises an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetraalkylammonium hydroxide and an oxidizing agent.
  2. A process according to claim 1, characterized in that the pH of said alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds is comprised between 8 and 12.
  3. A process according to one of claims 1 and 2, characterized in that the pH of said alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds is from 10.5 to 11.
  4. A process according to one of claims 1 to 3, characterized in that the average diameter of the abrasive particles of individualized colloidal silica particles of said composition is comprised between 12 nm and 100 nm.
  5. A process according to one of claims 1 to 4, characterized in that the average diameter of the colloidal silica abrasive particles of said composition is comprised between 35 nm and 50 nm.
  6. A process according to one of claims 1 to 5, characterized in that the concentration by weight in abrasive particles of said composition is comprised between 5% and 50%.
  7. A process according to one of claims 1 to 6, characterized in that the concentration by weight in abrasive particles of said composition is comprised between 25 and 35%.
  8. A process according to one of claims 1 to 7, characterized in that the stabilizing agent for individualized colloidal silica particles not linked to each other by siloxane bonds is tetramethylammonium hydroxide, tetraethylammonium hydroxide or tetrapropylammonium hydroxide.
  9. A process according to one of claims 1 to 8, characterized in that the quantity of tetralkylammonium hydroxide is comprised between 0.1% by weight and 1% by weight relative to the initial silica.
  10. A process according to one of claims 1 to 9, characterized in that the quantity of tetralkylammonium hydroxide is approximately 0.4% by weight relative to the initial silica.
  11. A process according to one of claims 1 to 10, characterized in that the oxidizing agent is chosen from chlorates, perchlorates, chlorites, iodates, nitrates, sulphates, persulphates, peroxides, ozonized water and hydrogen peroxide.
  12. A process according to one of claims 1 to 11, characterized in that the oxidizing agent is hydrogen peroxide.
  13. A process according to claim 12, characterized in that the quantity of hydrogen peroxide diluted to 30% in said abrasive composition is comprised between 0.5% and 10% by volume relative to the total of said abrasive composition.
  14. A process according to one of claims 12 and 13, characterized in that the quantity of hydrogen peroxide diluted to 30% in said abrasive composition is approximately 7.5% by volume relative to the total of said abrasive composition.
  15. Use of an abrasive composition comprising an alkaline aqueous suspension of individualized colloidal silica particles not linked to each other by siloxane bonds, a tetraalkylammonium hydroxide and an oxidizing agent, for mechanical chemical polishing of an aluminium or aluminium alloy conducting material used in the microelectronics semi-conductors industry.
EP00810129A 1999-02-18 2000-02-16 Process for mechanical chemical polishing of a layer of aluminium or aluminium alloy conducting material Expired - Lifetime EP1029907B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9902005A FR2789998B1 (en) 1999-02-18 1999-02-18 NOVEL MECHANICAL CHEMICAL POLISHING COMPOSITION OF A LAYER OF ALUMINUM OR ALUMINUM ALLOY CONDUCTIVE MATERIAL
FR9902005 1999-02-18

Publications (2)

Publication Number Publication Date
EP1029907A1 EP1029907A1 (en) 2000-08-23
EP1029907B1 true EP1029907B1 (en) 2003-07-02

Family

ID=9542207

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00810129A Expired - Lifetime EP1029907B1 (en) 1999-02-18 2000-02-16 Process for mechanical chemical polishing of a layer of aluminium or aluminium alloy conducting material

Country Status (14)

Country Link
US (1) US6386950B1 (en)
EP (1) EP1029907B1 (en)
JP (1) JP2000243734A (en)
KR (1) KR100685753B1 (en)
CN (1) CN1167109C (en)
AT (1) ATE244285T1 (en)
DE (1) DE60003591T2 (en)
DK (1) DK1029907T3 (en)
ES (1) ES2200804T3 (en)
FR (1) FR2789998B1 (en)
ID (1) ID24802A (en)
MY (1) MY128000A (en)
SG (1) SG97841A1 (en)
TW (1) TWI283703B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG108285A1 (en) * 2000-12-04 2005-01-28 Bayer Ag Polishing slurry for the chemical-mechanical polishing of metal and dielectric structures

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100367830B1 (en) * 2000-12-18 2003-01-10 제일모직주식회사 Composition for chemical mechanical polishing
DE10152993A1 (en) * 2001-10-26 2003-05-08 Bayer Ag Composition for the chemical mechanical polishing of metal and metal / dielectric structures with high selectivity
KR20040094758A (en) * 2002-03-04 2004-11-10 가부시키가이샤 후지미인코퍼레이티드 Polishing composition and method for forming wiring structure
JP4974447B2 (en) * 2003-11-26 2012-07-11 株式会社フジミインコーポレーテッド Polishing composition and polishing method
CN100427266C (en) * 2004-05-31 2008-10-22 中芯国际集成电路制造(上海)有限公司 Method and structure for aluminium chemical mechanical polishing and protective layer
US20080020680A1 (en) * 2006-07-24 2008-01-24 Cabot Microelectronics Corporation Rate-enhanced CMP compositions for dielectric films
DE102006039679B4 (en) * 2006-08-24 2011-02-10 Audi Ag Method for machining cylinder running surfaces of a cylinder crankcase or cylinder liners
CN101143996A (en) * 2006-09-15 2008-03-19 安集微电子(上海)有限公司 Chemical mechanical polishing fluid for polishing polycrystalline silicon
TWI408216B (en) * 2007-03-07 2013-09-11 Anji Microelectronics Co Ltd Application of Polishing Solution in Adjusting Polysilicon / Silica Selectivity Ratio
EP2268777A4 (en) * 2008-04-24 2011-11-23 Ppt Res Inc Stable aqueous slurry suspensions
EP2356192B1 (en) * 2008-09-19 2020-01-15 Cabot Microelectronics Corporation Barrier slurry for low-k dielectrics
CN102020975B (en) * 2010-07-21 2013-04-03 天津晶岭微电子材料有限公司 Preparation method of magnesium aluminum alloy surface chemically mechanical polishing solution
CN104736296B (en) * 2012-08-24 2018-08-28 艺康美国股份有限公司 The method for polishing sapphire surface
EP2969391B1 (en) 2013-03-15 2018-04-25 Ecolab USA Inc. Methods of polishing sapphire surfaces
CN104109481B (en) * 2014-06-26 2016-05-11 河北宇天昊远纳米材料有限公司 A kind of preparation method of sapphire substrate polishing solution
CN104109482B (en) * 2014-06-27 2016-04-20 河北宇天昊远纳米材料有限公司 A kind of aluminium alloy polishing fluid and preparation method thereof
US10586914B2 (en) 2016-10-14 2020-03-10 Applied Materials, Inc. Method of forming ultra-smooth bottom electrode surface for depositing magnetic tunnel junctions
CN106752969A (en) * 2016-11-22 2017-05-31 启东市清清蔬果农地股份专业合作社 A kind of polishing fluid of aluminum alloy casing

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69108546T2 (en) * 1991-05-28 1995-11-30 Rodel Inc Polishing paste made from silica with a low content of sodium and metals.
US5431777A (en) * 1992-09-17 1995-07-11 International Business Machines Corporation Methods and compositions for the selective etching of silicon
JPH07193034A (en) * 1993-03-26 1995-07-28 Toshiba Corp Polishing method
JP2606156B2 (en) * 1994-10-14 1997-04-30 栗田工業株式会社 Method for collecting abrasive particles
EP0779655A3 (en) * 1995-12-14 1997-07-16 International Business Machines Corporation A method of chemically-mechanically polishing an electronic component
MY133700A (en) * 1996-05-15 2007-11-30 Kobe Steel Ltd Polishing fluid composition and polishing method
US5866031A (en) * 1996-06-19 1999-02-02 Sematech, Inc. Slurry formulation for chemical mechanical polishing of metals
US5855811A (en) * 1996-10-03 1999-01-05 Micron Technology, Inc. Cleaning composition containing tetraalkylammonium salt and use thereof in semiconductor fabrication
FR2754937B1 (en) * 1996-10-23 1999-01-15 Hoechst France NOVEL MECHANICAL AND CHEMICAL POLISHING OF INSULATING MATERIAL LAYERS BASED ON SILICON OR SILICON DERIVATIVES
EP0853335A3 (en) * 1997-01-10 1999-01-07 Texas Instruments Incorporated Slurry and process for the mechano-chemical polishing of semiconductor devices
ATE214418T1 (en) * 1997-04-17 2002-03-15 Merck Patent Gmbh BUFFER SOLUTIONS FOR SUSPENSIONS USABLE FOR CHEMICAL-MECHANICAL POLISHING
US6083419A (en) * 1997-07-28 2000-07-04 Cabot Corporation Polishing composition including an inhibitor of tungsten etching

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG108285A1 (en) * 2000-12-04 2005-01-28 Bayer Ag Polishing slurry for the chemical-mechanical polishing of metal and dielectric structures

Also Published As

Publication number Publication date
MY128000A (en) 2007-01-31
ID24802A (en) 2000-08-24
KR100685753B1 (en) 2007-02-23
CN1264636A (en) 2000-08-30
FR2789998A1 (en) 2000-08-25
DE60003591D1 (en) 2003-08-07
FR2789998B1 (en) 2005-10-07
EP1029907A1 (en) 2000-08-23
KR20000058073A (en) 2000-09-25
SG97841A1 (en) 2003-08-20
CN1167109C (en) 2004-09-15
US6386950B1 (en) 2002-05-14
TWI283703B (en) 2007-07-11
ATE244285T1 (en) 2003-07-15
ES2200804T3 (en) 2004-03-16
DE60003591T2 (en) 2004-06-03
JP2000243734A (en) 2000-09-08
DK1029907T3 (en) 2003-10-13

Similar Documents

Publication Publication Date Title
EP1029907B1 (en) Process for mechanical chemical polishing of a layer of aluminium or aluminium alloy conducting material
US5783489A (en) Multi-oxidizer slurry for chemical mechanical polishing
EP1090083B1 (en) Chemical mechanical polishing slurry useful for copper/tantalum substrates
US5993686A (en) Fluoride additive containing chemical mechanical polishing slurry and method for use of same
US6063306A (en) Chemical mechanical polishing slurry useful for copper/tantalum substrate
KR100581649B1 (en) Composition and Method for Polishing in Metal CMP
US6033596A (en) Multi-oxidizer slurry for chemical mechanical polishing
RU2356926C2 (en) Abrasive particles for mechanical polishing
US7381648B2 (en) Chemical mechanical polishing slurry useful for copper substrates
US6039891A (en) Multi-oxidizer precursor for chemical mechanical polishing
US20030168627A1 (en) Slurry and method for chemical mechanical polishing of metal structures including refractory metal based barrier layers
US20080148652A1 (en) Compositions for chemical mechanical planarization of copper
US11066575B2 (en) Chemical mechanical planarization for tungsten-containing substrates
EP0982766A1 (en) Process for chemo-mechanical polishing of a copper-based material layer
AU9338401A (en) Polishing slurry for the chemical-mechanical polishing of metal and dielectric structures
KR20040089631A (en) Process for chemical-mechanical polishing of metal substrates
WO2001030928A1 (en) Chemical mechanical polishing compositions and systems

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

17P Request for examination filed

Effective date: 20001216

AKX Designation fees paid

Free format text: AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: CLARIANT FINANCE (BVI) LIMITED

17Q First examination report despatched

Effective date: 20020529

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20030702

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: CH

Ref legal event code: NV

Representative=s name: CLARIANT INTERNATIONAL LTD.

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REF Corresponds to:

Ref document number: 60003591

Country of ref document: DE

Date of ref document: 20030807

Kind code of ref document: P

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031002

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031002

REG Reference to a national code

Ref country code: SE

Ref legal event code: TRGR

ET Fr: translation filed
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040216

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040228

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2200804

Country of ref document: ES

Kind code of ref document: T3

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20040405

REG Reference to a national code

Ref country code: HK

Ref legal event code: WD

Ref document number: 1030235

Country of ref document: HK

REG Reference to a national code

Ref country code: CH

Ref legal event code: PUE

Owner name: AZ ELECTRONIC MATERIALS USA CORP.

Free format text: CLARIANT FINANCE (BVI) LIMITED#CITCO BUILDING, WICKHAMS CAY#ROAD TOWN, TORTOLA (VG) -TRANSFER TO- AZ ELECTRONIC MATERIALS USA CORP.#70 MEISTER AVENUE#SOMERVILLE, NJ 08876 (US)

REG Reference to a national code

Ref country code: GB

Ref legal event code: 732E

NLS Nl: assignments of ep-patents

Owner name: AZ ELECTRONIC MATERIALS USA CORP.

REG Reference to a national code

Ref country code: FR

Ref legal event code: TP

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DK

Payment date: 20060109

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 20060203

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20060215

Year of fee payment: 7

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070217

REG Reference to a national code

Ref country code: DK

Ref legal event code: EBP

EUG Se: european patent has lapsed
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070228

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20070217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070217

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 16

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: SCHNEIDER FELDMANN AG PATENT- UND MARKENANWAEL, CH

Ref country code: CH

Ref legal event code: PUE

Owner name: MERCK PATENT GMBH, DE

Free format text: FORMER OWNER: AZ ELECTRONIC MATERIALS USA CORP., US

REG Reference to a national code

Ref country code: DE

Ref legal event code: R082

Ref document number: 60003591

Country of ref document: DE

Representative=s name: PATENTANWAELTE ISENBRUCK BOESL HOERSCHLER LLP, DE

REG Reference to a national code

Ref country code: GB

Ref legal event code: 732E

Free format text: REGISTERED BETWEEN 20150205 AND 20150211

REG Reference to a national code

Ref country code: FR

Ref legal event code: TP

Owner name: MERCK PATENT GMBH, DE

Effective date: 20150204

REG Reference to a national code

Ref country code: AT

Ref legal event code: PC

Ref document number: 244285

Country of ref document: AT

Kind code of ref document: T

Owner name: MERCK PATENT GMBH, DE

Effective date: 20150123

REG Reference to a national code

Ref country code: NL

Ref legal event code: SD

Effective date: 20150324

REG Reference to a national code

Ref country code: DE

Ref legal event code: R082

Ref document number: 60003591

Country of ref document: DE

Representative=s name: PATENTANWAELTE ISENBRUCK BOESL HOERSCHLER LLP, DE

Effective date: 20150223

Ref country code: DE

Ref legal event code: R081

Ref document number: 60003591

Country of ref document: DE

Owner name: MERCK PATENT GMBH, DE

Free format text: FORMER OWNER: AZ ELECTRONIC MATERIALS USA CORP. (N.D.GES.D. STAATES DELAWARE), SOMERVILLE, N.J., US

Effective date: 20150223

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: BRAUNPAT BRAUN EDER AG, CH

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 17

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 18

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 20170110

Year of fee payment: 18

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20170112

Year of fee payment: 18

Ref country code: CH

Payment date: 20170214

Year of fee payment: 18

Ref country code: FI

Payment date: 20170209

Year of fee payment: 18

Ref country code: DE

Payment date: 20170207

Year of fee payment: 18

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20170125

Year of fee payment: 18

Ref country code: IE

Payment date: 20170209

Year of fee payment: 18

Ref country code: GB

Payment date: 20170215

Year of fee payment: 18

Ref country code: BE

Payment date: 20161228

Year of fee payment: 18

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20170221

Year of fee payment: 18

REG Reference to a national code

Ref country code: CH

Ref legal event code: PCAR

Free format text: NEW ADDRESS: HOLEESTRASSE 87, 4054 BASEL (CH)

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 60003591

Country of ref document: DE

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: NL

Ref legal event code: MM

Effective date: 20180301

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 244285

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180216

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20180216

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180216

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20180228

Ref country code: BE

Ref legal event code: PD

Owner name: MERCK PATENT GMBH; DE

Free format text: DETAILS ASSIGNMENT: CHANGE OF OWNER(S), AFFECTATION / CESSION; FORMER OWNER NAME: AZ ELECTRONIC MATERIALS USA CORP.

Effective date: 20150121

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180216

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180228

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180228

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20181031

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180301

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180216

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180901

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180216

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180228

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180216

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180228